HRID47923

反应详情

EQUATION

反应方程式

HRID 47923 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

4-(4-Methoxyphenyl)-2-oxo-4-oxazoline (1.00 g), methyl acrylate (0.94 mL) was dissolved in toluene (20 mL) and boron trifluoride etherate (1.31 mL) was added. The obtained mixture was heated to 90° C., and after stirring for 2 h, the solvent was concentrated under reduced pressure to give an oily substance. The obtained oily substance was subjected to silica gel column chromatography and eluted with n-hexane-ethyl acetate (1:1). The solvent was evaporated and the obtained oil was crystallized from ethanol. Isopropyl ether (10 mL) was added and the mixture was stirred at not higher than 5° C. for 1 h. The crystals were collected by filtration and washed with isopropyl ether to give the title compound (0.30 g; yield 20.7%) as gray-white crystals.

WORKUP

后处理

  1. concentrationthe solvent was concentrated under reduced pressure
  2. customto give an oily substance
  3. washeluted with n-hexane-ethyl acetate (1:1)
  4. customThe solvent was evaporated
  5. customthe obtained oil was crystallized from ethanol
  6. additionIsopropyl ether (10 mL) was added
  7. stirringthe mixture was stirred at not higher than 5° C. for 1 h
  8. filtrationThe crystals were collected by filtration
  9. washwashed with isopropyl ether